CN217189556U - Polyvinyl chloride resin heat stability refining production process device - Google Patents
Polyvinyl chloride resin heat stability refining production process device Download PDFInfo
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- CN217189556U CN217189556U CN202220275144.8U CN202220275144U CN217189556U CN 217189556 U CN217189556 U CN 217189556U CN 202220275144 U CN202220275144 U CN 202220275144U CN 217189556 U CN217189556 U CN 217189556U
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Abstract
The utility model relates to a polyvinyl chloride resin thermostability refines production process units, include terminator A line, terminator B line and go into the cauldron circuit: the device comprises a terminator storage tank A, a terminator feeding pump A, a terminator flow meter A and a terminator regulating valve A which are connected in sequence; the system comprises a terminator cut-off valve A, a terminator storage tank B, a terminator feeding pump B, a terminator flow meter B and a terminator regulating valve B; the polymerization kettle comprises a terminator stop valve B, a kettle feeding pipeline, a feeding main regulating valve, a feeding main stop valve and kettle feeding stop valves, wherein two groups of different terminators with different dosages are added into a polymerization kettle in two batches, an emulsion terminator and an oil-soluble terminator are respectively added into each batch, the low-speed uniform rotation of polymerization stirring is controlled, the reaction temperature and the discharge pressure are controlled, the terminator is added in a composite mode, the performance of the polyvinyl chloride resin is stabilized, the thermal stability of the polyvinyl chloride resin is improved, and the aging whiteness index is particularly beneficial.
Description
Technical Field
The utility model belongs to the technical field of polyvinyl chloride production refining production, concretely relates to polyvinyl chloride resin heat stability refining production process device.
Background
The production process of polyvinyl chloride is characterized by that the monomer fed from vinyl chloride process is passed through a polymerization still, and added with various assistants to make polymerization reaction to produce polyvinyl chloride slurry, and the VCM not participating in polymerization reaction in the slurry is removed from stripping position, and then passed through drying position, and its water content is removed and controlled at less than 0.5%, and then the product can be packaged and sold by packaging position. Thermal stability is an important performance index of polyvinyl chloride (PVC) resin, and directly influences the application range and service life of PVC products, so PVC resin production enterprises and processing enterprises pay great attention to the thermal stability of PVC.
General special polymerization equipment for polyvinyl chloride comprises more polymerization kettles for carrying out high speed cultivation at 70m and 108 m, and the stirring is a two-layer three-leaf sweepback type; the production process and flow mainly comprise two parts; the first part is fed with isothermal water, and the other part is fed with conventional water and heated to the set reaction temperature of the polymerization kettle. The process is explained by an isothermal water feeding mode, the wall of a polymerization kettle is coated before feeding, the reaction temperature is set after raw materials and auxiliary materials are added, the polymerization kettle reaches the discharging condition after the set pressure drop is reached, and a terminator is added to terminate the polymerization reaction. When the polymerization reaction reaches a certain discharge condition, one of the terminating agents is generally added to achieve the purpose of terminating the reaction, and particularly when the production is abnormal, the terminating agent can play a role in safely terminating the reaction to a certain extent. When the characteristics in the use experience of the terminating agent are combined, the two terminating agents are simultaneously added in the composite adding process, the characteristics of the oil-soluble terminating agent and the emulsion terminating agent are synthesized through experiments, the performance of the polyvinyl chloride resin can be stabilized, the thermal stability of the polyvinyl chloride resin is improved by adopting the composite adding terminating agent, the ageing whiteness index is particularly beneficial, and the thermal performance and the ageing whiteness of a post-processed product are improved.
The problems that exist at present are:
1. the potential safety hazard exists to the safety in production to two kinds of different materials of nature of single line addition, and the layering is easy in the material density difference feeding pipeline, and control personnel manual operation is frequent during the feeding, and long-term frequent operation is tired easily and is produced the mistake.
2. The addition amount of the terminating agent is not enough, the free radical of the chloroethylene is not completely terminated or sheared, and the polymerization reaction of the chloroethylene gives out heat, thereby causing certain influence on safe production.
Disclosure of Invention
The utility model provides a not enough to prior art, the utility model aims at providing a polyvinyl chloride resin heat stability refines production process units, through this set of refined production process, there is the hidden danger to the safety in production to solve the inequality material of two kinds of properties to and solved because of easy layering in the different charging line of material density, control personnel manual operation is frequent when reinforced simultaneously, the incomplete problem of terminator addition, improve polyvinyl chloride resin's heat stability greatly, especially to the promotion of ageing whiteness index, especially a polyvinyl chloride resin heat stability refines production process units.
The invention comprises a polymerization feeding process, a polymerization reaction process and a polymerization discharging process, and is characterized in that the charging procedure of the polymerization process comprises the following steps: general SG-5 type PVC resin 70m polymeric kettle, set up polymerization control temperature as first reaction temperature, pressure setting first reaction pressure. Feeding vinyl chloride monomer and soft water according to a certain proportion, adding a certain amount of dispersant and initiator with certain purity, adding the mixture into a polymerization kettle through a closed feeding system, continuously stirring the mixture while adding the materials, reacting the mixture for a set time, and adding two groups of different terminators with different dosages into the polymerization kettle in two batches when the pressure drop of the kettle reaches a preset value: adding a certain amount of emulsion terminator into the first batch, delaying for a certain time after adding, adding a certain amount of oil-soluble terminator, controlling the polymerization stirring to rotate at a low speed and a uniform speed, setting a second reaction temperature for the reaction temperature setting transition, and setting a second reaction pressure for the pressure; adding a certain amount of emulsion terminator into the second batch, delaying for a certain time after adding, adding a certain amount of oil-soluble terminator, controlling the polymerization stirring to rotate at a low speed and a uniform speed, setting a third reaction temperature for the setting transition of the reaction temperature, and setting a third reaction pressure for the pressure; continuously stirring for a certain time and then discharging.
In the above process, a DCS control system accurately controls a feeding and feeding starting program, when a certain amount of terminator adding flow is selected, an adding lead is set in advance, when the adding amount is close, a terminator regulating valve is adjusted to be added to a small valve position, when the entering amount is reached, and when 98% of mass dosage is finished in advance, a terminator stop valve, a terminator regulating valve and a terminator feeding pump are closed, washing water is added twice, and the washing dosage is subtracted from the feeding dosage of the total amount of soft water to be fed.
In the above working procedures, when any terminator feeding production line is abnormal, the system prompts an alarm prompt message, if the terminator A enters the kettle abnormally, a terminator B line feeding program is automatically started, and the accumulated data A and the total adding amount are used as difference values to be used as the feeding amount of the terminator B line; similarly, if the line feeding of the terminator B is abnormal, a line feeding program of the terminator A is automatically started, and the difference value is made by the accumulated data of the line B and the total adding amount and is used as the line feeding amount of the terminator A.
When the production is normal in the above procedures, the terminator storage tank has enough liquid level, the number of the feeding kettle is selected, the terminator feeding pump is started to open the feeding main cut-off valve, the branch cut-off valve is opened, the flowmeter measures, and the branch cut-off valve, the main cut-off valve and the pump are closed and stopped to start after the target is reached.
The terminator of the invention is most preferably prepared by the following processing method:
carrying out 70m general SG-5 type PVC resin cultivation by using a polymerization kettle, and predicting to add 25.00t of vinyl chloride monomer; 31.00t ton of soft water, setting the reaction temperature to be 57.5 ℃, controlling the reaction pressure to be 0.80MPa of saturated vapor pressure, and adding a pre-weighed dispersant with a molecular formula: the purity of [ C2H4O ] n is 86-90mom/mol%, and the addition amount is the proportion of the total amount of vinyl chloride monomer: 200 ppm; adding a pre-measured initiator, wherein the content of the 1-bis- (2-ethylhexyl) peroxydicarbonate is less than or equal to 52 percent; 4, the content of the peroxyneodecanoic acid cumyl ester is less than or equal to 52 percent according to the proportion of 2: 1, adding the materials in the proportion of the total amount of the vinyl chloride monomer, wherein the materials are respectively as follows: 400 ppm; 200 ppm; the reaction is carried out for 240 minutes, and the pressure drop of the kettle reaches the preset value of 0.05 Mpa.
In the above process, two groups of different terminating agents with different dosages are added into a polymerization kettle in two batches: adding a certain amount of emulsion terminator into the first batch, delaying for a certain time after adding, adding a certain amount of oil-soluble terminator, controlling the polymerization stirring to rotate at a low speed and a uniform speed, setting a second reaction temperature for the reaction temperature setting transition, and setting a second reaction pressure for the pressure; adding a certain amount of emulsion terminator into the second batch, delaying for a certain time after adding, adding a certain amount of oil-soluble terminator, controlling the polymerization stirring to rotate at a low speed and a uniform speed, setting a third reaction temperature for the set transition at the reaction temperature, and setting a third reaction pressure at the pressure; continuously stirring for a certain time and then discharging. The essential components of the emulsion terminator are antioxidant with the concentration of 40 percent, and the main components of the oil-soluble terminator are as follows: epoxidized soybean oil and a high-efficiency terminator, wherein the concentration of the epoxidized soybean oil and the high-efficiency terminator is 40%, 185 ppm of an emulsion terminator is added in the first batch, the time delay is carried out for 2-3 minutes after the addition, 175ppm of an oil-soluble terminator is added, and the time delay is carried out for 3-5 minutes after the addition; stirring at a low speed of 100-110 rpm, wherein the reaction temperature is 57.5 +/-0.2 ℃, and the pressure is 0.68-0.75 MPa; adding 215ppm of emulsion terminator into the second batch, delaying for 2-3 minutes after adding, and then adding 225 ppm of oil-soluble terminator; stirring at a low speed of 90-100 rpm, wherein the reaction temperature is 57.3 +/-0.2 ℃, and the pressure is 0.68-0.73 MPa; continuously stirring for 5 minutes and discharging.
The production device realized by the polyvinyl chloride resin thermal stability refining production process method comprises a terminator A line, a terminator B line and a kettle entering line: terminator line a: the system comprises a terminator storage tank A, a terminator feeding pump A, a terminator flow meter A and a terminator regulating valve A which are connected in sequence; a terminator cut-off valve A; terminator line B: the device comprises a terminator storage tank B, a terminator feeding pump B, a terminator flow meter B and a terminator regulating valve B which are connected in sequence; a terminator cut-off valve B; entering a kettle circuit: comprises a kettle feeding pipeline, a feeding main regulating valve, a feeding main cut-off valve and kettle feeding cut-off valves.
The terminator A line and the terminator B line are added with different types of assistants according to production requirements, and different assistants can be added in batches and in different dosages according to production requirements.
The feeding main regulating valve and the feeding cut-off valve are sequentially arranged and opened, when the feeding main regulating valve and the feeding cut-off valve are closed, the feeding cut-off valve and the feeding main regulating valve are reversely closed, when a setting program is abnormal, the accumulated total amount of a terminator A line and a terminator B line is interlocked with the feeding main regulating valve 31 and the feeding main cut-off valve 32, and an automatic starting and stopping program is set by a DCS control system.
The feeding cut-off valves of all the kettles are uniformly distributed on all the kettles and are mainly used for controlling the adding amount of the terminating agent entering the kettles and the operation safety.
And the instantaneous metering value and the accumulated metering value of the terminating agent flowmeter A and the terminating agent flowmeter B are introduced into the DCS control system by signal lines.
Stopping and starting of various parts and feedback signals are introduced into the DCS control system through signal lines, and operation convenience and accuracy of the control system are improved.
The various terminating agents are prepared according to a certain temperature and are pumped into a terminating agent storage tank A and a terminating agent storage tank B, and the various terminating agents are sequentially connected through a terminating agent storage tank A, a terminating agent feeding pump A, a terminating agent flow meter A and a terminating agent regulating valve A by a pipeline; a terminator cut-off valve A; the system comprises a terminator storage tank B, a terminator feeding pump B, a terminator flow meter B and a terminator regulating valve B which are connected in sequence; a terminator cut-off valve B; the addition amount of the terminator is accurately controlled through the feeding pipeline, the feeding main regulating valve, the feeding main stop valve and the corresponding feeding amount of the terminator, so that various substances with different properties of the terminator are favorably controlled, various termination reaction properties are uniform and suitable, after feeding is finished, high-pressure water is started to flush all feeding pipes to the feeding pipeline of the kettle, the feeding of the terminator is ensured to be more complete and accurate, and in the feeding process, the stirring is uniformly carried out at a low speed, so that the thermal stability, especially the aging whiteness performance, of the resin is effectively improved.
The feeding procedure is described as follows:
step 1, selecting a kettle number, setting automatic flow feeding, setting an adding batch and adding any terminator feeding amount, setting a feeding advance, setting the amount of valves closed in advance, setting the amount of flushing water entering a kettle, setting any time in the middle of a program, and pausing or stopping at proper time according to actual production conditions;
step 2, starting a terminator A line, sequentially judging whether the liquid level of a terminator storage tank A is greater than the lowest limit, starting a program A line, starting a terminator feed pump A, resetting a terminator flowmeter A, starting accumulation, and starting a terminator regulating valve A; opening a terminator cut-off valve A, feeding cut-off valves to kettles, judging that the feeding amount is close to 85% of the total feeding amount, adjusting the valve position of a terminator adjusting valve A to 90%, judging that the feeding amount is close to 95% of the total feeding amount, closing the terminator cut-off valve A and the terminator adjusting valve A in an adjusting procedure, and delaying for 2-3 minutes after feeding;
step 3, starting a terminator B line, sequentially judging whether the liquid level of the terminator storage tank B is greater than the lowest limit, starting a program B line, starting a terminator feed pump B, resetting a terminator flow meter B, starting accumulation, and starting a terminator regulating valve B; opening a terminator cut-off valve B, feeding a material to each kettle, cutting off the material, judging that the feeding amount is close to 85% of the total feeding amount, adjusting the valve position of a terminator regulating valve B to 90%, judging that the feeding amount is close to 95% of the total feeding amount, closing the terminator cut-off valve B and the terminator regulating valve B in an adjusting procedure, and delaying for 3-5 minutes after feeding;
step 5, starting the feeding amount of the second batch and a corresponding program on the line A of the terminator, and delaying for 2-3 minutes after adding;
step 5, starting the feeding dosage of the second batch and a corresponding program by using a terminator line B; delay time 5 minutes.
Step 6, setting a reaction temperature to be 57.2 ℃ in the processes from feeding to adding of the terminator, stirring at a low speed for 100-110 rpm after the addition of the terminator in the first batch is finished, wherein the reaction temperature is 57.5 +/-0.2 ℃, and the pressure is set to be 0.68-0.75 MPa; after the second batch is added, stirring at a low speed of 90-100 rpm, wherein the reaction temperature is 57.3 +/-0.2 ℃, and the pressure is 0.68-0.73 MPa; continuously stirring for 5 minutes and discharging.
And 7, finishing the steps, and restoring all the switches to be reset to the original positions for the next starting.
Compared with the prior art, the utility model discloses it increases redundant feeding system to have taken terminator charging system on terminator charging process, it is automatic to improve polyvinyl chloride production feeding system, improve the product quality, avoid terminator charging system trouble to cause the influence to safety in production, and multibatch multiunit formula terminator joining mode, control joining time and reaction temperature and pressure, make polymerization after organic processing can be compatible with vinyl chloride monomer under dispersant, initiating agent and certain auxiliary agent system with the help of stirring process messenger, the process of adding is gradually delayed, make polymerization take place copolymerization more perfectly, it has the hidden danger to safety in production to have solved the inequality material of two kinds of properties, and solved because of the easy layering in the different charging line of material density, control personnel manual operation is frequent when reinforced simultaneously, the utility model discloses a method for preparing a novel compound material, The addition of the terminating agent is not complete, the thermal stability of the polyvinyl chloride resin is greatly improved, and particularly the aging whiteness index is improved.
Drawings
Fig. 1 is a schematic view of the device of the present invention.
In fig. 1: 10 is a terminator storage tank A; 11 is a terminator charging pump A; 12 is a terminator flowmeter A; 13 is a terminator regulating valve A; 14 is a terminator cut-off valve A;
20 is a terminator storage tank B; 21 is a terminator charging pump B; 22 is terminator flow meter B; 23 is a terminator regulating valve B; 24 is a terminator cut-off valve B;
30 is a feeding pipeline into the kettle; 31 is a charging main regulating valve; and 32 is a feeding total shut-off valve.
Detailed Description
For a more detailed description of the present invention, reference is made to the accompanying drawings, which show, by way of illustration:
in fig. 1, the technical solution of the present invention is: the production process method comprises a polymerization feeding process, a polymerization reaction process and a polymerization discharging process, and is characterized in that the feeding procedure of the polymerization process is as follows: general SG-5 type PVC resin 70m polymeric kettle, set up polymerization control temperature as first reaction temperature, pressure setting first reaction pressure. Feeding vinyl chloride monomer and soft water according to a certain proportion, adding a certain amount of dispersant and initiator with certain purity, adding the mixture into a polymerization kettle through a closed feeding system, continuously stirring the mixture while adding the materials, reacting the mixture for a set time, and adding two groups of different terminators with different dosages into the polymerization kettle in two batches when the pressure drop of the kettle reaches a preset value: adding a certain amount of emulsion terminator into the first batch, delaying for a certain time after adding, adding a certain amount of oil-soluble terminator, controlling the polymerization stirring to rotate at a low speed and a uniform speed, setting a second reaction temperature for the set transition at the reaction temperature, and setting a second reaction pressure at the pressure; adding a certain amount of emulsion terminator into the second batch, delaying for a certain time after adding, adding a certain amount of oil-soluble terminator, controlling the polymerization stirring to rotate at a low speed and a uniform speed, setting a third reaction temperature for the set transition at the reaction temperature, and setting a third reaction pressure at the pressure; continuously stirring for a certain time and then discharging.
In the above process, a DCS control system accurately controls a feeding and feeding starting program, when a certain amount of terminator adding flow is selected, an adding lead is set in advance, when the adding amount is close, a terminator regulating valve is adjusted to be added to a small valve position, when the entering amount is reached, and when 98% of mass dosage is finished in advance, a terminator stop valve, a terminator regulating valve and a terminator feeding pump are closed, washing water is added twice, and the washing dosage is subtracted from the feeding dosage of the total amount of soft water to be fed.
In the above working procedures, when any terminator feeding production line is abnormal, the system prompts an alarm prompt message, if the terminator A enters the kettle abnormally, a terminator B line feeding program is automatically started, and the accumulated data A and the total adding amount are used as difference values to be used as the feeding amount of the terminator B line; similarly, if the line feeding of the terminator B is abnormal, a line feeding program of the terminator A is automatically started, and the difference value is made by the accumulated data of the line B and the total adding amount and is used as the line feeding amount of the terminator A.
When the production is normal in the above procedures, the terminator storage tank has enough liquid level, the number of the feeding kettle is selected, the terminator feeding pump is started to open the feeding main cut-off valve, the branch cut-off valve is opened, the flowmeter measures, and the branch cut-off valve, the main cut-off valve and the pump are closed and stopped to start after the target is reached.
The terminator of the invention is most preferably prepared by the following processing method:
carrying out 70m general SG-5 type PVC resin cultivation by using a polymerization kettle, and predicting to add 25.00t of vinyl chloride monomer; 31.00t ton of soft water, setting the reaction temperature to be 57.5 ℃, controlling the reaction pressure to be 0.80MPa of saturated vapor pressure, and adding a pre-weighed dispersant with a molecular formula: the purity of [ C2H4O ] n is 86-90mom/mol%, and the addition amount is the proportion of the total amount of vinyl chloride monomer: 200 ppm; adding a pre-measured initiator, wherein the content of the 1-bis- (2-ethylhexyl) peroxydicarbonate is less than or equal to 52 percent; 4, the content of the peroxyneodecanoic acid cumyl ester is less than or equal to 52 percent according to the proportion of 2: 1, adding the materials in the proportion of the total amount of the vinyl chloride monomer, wherein the materials are respectively as follows: 400 ppm; 200 ppm; the reaction time is 240 minutes, and the pressure drop of the kettle reaches the preset value of 0.05 Mpa.
In the above process, two groups of different terminating agents with different dosages are added into a polymerization kettle in two batches: adding a certain amount of emulsion terminator into the first batch, delaying for a certain time after adding, adding a certain amount of oil-soluble terminator, controlling the polymerization stirring to rotate at a low speed and a uniform speed, setting a second reaction temperature for the reaction temperature setting transition, and setting a second reaction pressure for the pressure; adding a certain amount of emulsion terminator into the second batch, delaying for a certain time after adding, adding a certain amount of oil-soluble terminator, controlling the polymerization stirring to rotate at a low speed and a uniform speed, setting a third reaction temperature for the set transition at the reaction temperature, and setting a third reaction pressure at the pressure; continuously stirring for a certain time and then discharging. The essential components of the emulsion terminator are antioxidant with the concentration of 40 percent, and the main components of the oil-soluble terminator are as follows: epoxidized soybean oil and a high-efficiency terminator, wherein the concentration of the epoxidized soybean oil and the high-efficiency terminator is 40%, 185 ppm of an emulsion terminator is added in the first batch, the time delay is carried out for 2-3 minutes after the addition, 175ppm of an oil-soluble terminator is added, and the time delay is carried out for 3-5 minutes after the addition; stirring at a low speed of 100-110 rpm, wherein the reaction temperature is 57.5 +/-0.2 ℃, and the pressure is 0.68-0.75 MPa; adding 215ppm of emulsion terminator into the second batch, delaying for 2-3 minutes after adding, and then adding 225 ppm of oil-soluble terminator; stirring at a low speed of 90-100 rpm, wherein the reaction temperature is 57.3 +/-0.2 ℃, and the pressure is 0.68-0.73 MPa; continuously stirring for 5 minutes and discharging.
The production device realized by the polyvinyl chloride resin thermal stability refining production process method comprises a terminator A line, a terminator B line and a kettle entering line: terminator line a: comprises a terminator storage tank A10, a terminator charging pump A11, a terminator flow meter A12 and a terminator regulating valve A13 which are connected in sequence; terminator cutoff valve a 14; terminator line B: comprises a terminator storage tank B20, a terminator charging pump B21, a terminator flow meter B22 and a terminator regulating valve B23 which are connected in sequence; terminator cutoff valve B24; entering a kettle circuit: comprises a feeding pipeline 30, a feeding main regulating valve 31, a feeding main cut-off valve 32 and feeding cut-off valves for feeding each kettle into the kettle.
The terminator A line and the terminator B line are added with different types of assistants according to production requirements, and different assistants can be added in batches and in different dosages according to production requirements.
The feeding main regulating valve and the feeding cut-off valve are sequentially arranged and opened, when the feeding main regulating valve and the feeding cut-off valve are closed, the feeding cut-off valve and the feeding main regulating valve are reversely closed, when a setting program is abnormal, the accumulated total amount of a terminator A line and a terminator B line is interlocked with the feeding main regulating valve 31 and the feeding main cut-off valve 32, and an automatic starting and stopping program is set by a DCS control system.
The feeding cut-off valves of all the kettles are uniformly distributed on all the kettles and are mainly used for controlling the adding amount of the terminating agent entering the kettles and the operation safety.
And the instantaneous metering value and the accumulated metering value of the terminator flowmeter A12 and the terminator flowmeter B22 are introduced into the DCS control system through signal lines.
Stopping and starting of various parts and feedback signals are introduced into the DCS control system through signal lines, and operation convenience and accuracy of the control system are improved.
The various terminators are prepared according to a certain temperature and are pumped into a terminator storage tank A and a terminator storage tank B, and the various terminators are sequentially connected through a pipe inlet pipeline, a terminator storage tank A10, a terminator feed pump A11, a terminator flow meter A12 and a terminator regulating valve A13; terminator cutoff valve a 14; the system is characterized by comprising a terminator storage tank B20, a terminator charging pump B21, a terminator flow meter B22 and a terminator regulating valve B23 which are connected in sequence; terminator cutoff valve B24; the addition amount of the terminator is accurately controlled through the feeding pipeline 30, the feeding main regulating valve 31, the feeding main stop valve 32 and the corresponding feeding amount, so that various substances with different properties of the terminator are favorably controlled, various termination reaction properties are uniform and suitable, after the feeding is finished, all feeding pipes are flushed to the feeding pipeline of the kettle by high-pressure water, the feeding of the terminator is ensured to be more complete and accurate, in addition, in the feeding process, the stirring is uniformly carried out at a low speed, and the thermal stability, especially the aging whiteness performance of the resin is effectively improved.
The feeding procedure is described as follows:
step 1, selecting a kettle number, setting automatic flow feeding, setting an adding batch and adding any terminator feeding amount, setting a feeding advance, setting the amount of valves closed in advance, setting the amount of flushing water entering a kettle, setting any time in the middle of a program, and pausing or stopping at proper time according to actual production conditions;
step 2, starting a terminator A line, sequentially judging whether the liquid level of the terminator storage tank A10 is greater than the lowest limit, starting a program A line, starting a terminator feed pump A11 and a terminator flow meter A12, clearing, starting accumulation, and starting a terminator regulating valve A13; opening a terminator cut-off valve A14, feeding cut-off valves to kettles, judging that the feeding amount is close to 85% of the total feeding amount, adjusting the valve position of a terminator adjusting valve A13 to 90%, judging that the feeding amount is close to 95% of the total feeding amount, closing the terminator cut-off valve A14 and the terminator adjusting valve A13 in the adjusting procedure, and delaying for 2-3 minutes after feeding;
step 3, starting a terminator B line, sequentially judging whether the liquid level of the terminator storage tank B20 is greater than the lowest limit, starting a program B line, starting a terminator feed pump B21 and a terminator flowmeter B22, clearing, starting accumulation, and starting a terminator regulating valve B23; opening a terminator cut-off valve B24, feeding cut-off valves to kettles, judging that the feeding amount is close to 85% of the total feeding amount, adjusting a valve position of a terminator adjusting valve B13 to 90%, judging that the feeding amount is close to 95% of the total feeding amount, closing a terminator cut-off valve B24 and a terminator adjusting valve B23 in an adjusting procedure, and delaying for 3-5 minutes after feeding;
step 4, starting the feeding dosage of the second batch and a corresponding program by using a terminator A line, and delaying for 2-3 minutes after adding;
step 5, starting the feeding dosage of the second batch and a corresponding program by using a terminator line B; delay time 5 minutes.
Step 6, setting a reaction temperature to be 57.2 ℃ in the processes from feeding to adding of the terminator, stirring at a low speed for 100-110 rpm after the addition of the terminator in the first batch is finished, wherein the reaction temperature is 57.5 +/-0.2 ℃, and the pressure is set to be 0.68-0.75 MPa; after the second batch is added, stirring at a low speed of 90-100 rpm, wherein the reaction temperature is 57.3 +/-0.2 ℃, and the pressure is 0.68-0.73 MPa; continuously stirring for 5 minutes and discharging.
And 7, finishing the steps, and restoring all the switches to be reset to the original positions for the next starting.
Compared with the prior art, the invention adopts the terminator charging A system to add the redundant charging system B system in the terminator charging process, improves the automation of the polyvinyl chloride production charging system, improves the product quality, avoids the influence of the fault of the terminator charging system on the safety production, and the adding mode of the multi-batch multi-combination type terminator controls the adding time, the reaction temperature and the pressure, the feeding doses of the first batch and the second batch and the corresponding programs are started by the terminator A line, the delay time after adding is different, the feeding doses of the first batch and the second batch and the corresponding programs are started by the terminator B line, the delay time after adding is different, setting the reaction temperature to be 57.2 ℃ in the processes from feeding to adding the terminator, stirring at a low speed for 100-110 rpm after the addition of the terminator in the first batch is finished, wherein the reaction temperature is 57.5 +/-0.2 ℃, and the pressure is set to be 0.68-0.75 MPa; after the second batch is added, stirring at a low speed of 90-100 rpm, wherein the reaction temperature is 57.3 +/-0.2 ℃, and the pressure is 0.68-0.73 MPa; continuously stirring for 5 minutes, discharging, and recovering all switches to reset to the original position after finishing the program so as to prepare for the next start. The polymerization reaction after organic treatment can make the soft water and the vinyl chloride monomer compatible under a dispersant, an initiator and a certain assistant system, and the polymerization reaction is added in a delayed and gradual manner by virtue of a stirring process, so that the copolymerization reaction is more perfectly promoted, the hidden danger of two substances with different properties on safety production is solved, the problems that the feeding pipelines are easy to layer due to different material densities, manual operation of control personnel is frequent during feeding, and the addition amount of the terminator is not complete are solved, the thermal stability of the polyvinyl chloride resin is greatly improved, and particularly the aging whiteness index is improved.
The following embodiments are described with reference to the above process and device structure characteristics:
example 1, a process for thermally stable, refined production of polyvinyl chloride resin, comprising the steps of general 70m high-speed (SG-5) PVC resin polymerizing vessel under agitation for two-layer three-leaf sweepback; 25.00t of vinyl chloride monomer is expected to be added; 31.00t of soft water, 57.5 ℃ of reaction temperature and 0.80MPa of saturated vapor pressure, and adding a pre-measured dispersant (molecular formula: [ C2H4O ] n with the purity of 86-90mom/mol% and the addition of 200 ppm).
Another example differs in that the purity is 74-83mom/mol% and the amount added is 200 ppm.
Another example differs in that the purity is 38-45 mom/mol%; the amount added was 320 ppm.
Another embodiment is different in that a pre-measured initiator (di-2-ethylhexyl 1 peroxydicarbonate) is added to the reactor (the content is less than or equal to 52 percent; 4 peroxyneodecanoic acid cumyl ester [ the content is less than or equal to 52 percent and the proportion is 2: 1, adding in proportion of: 400 ppm; 200 ppm).
The other embodiment is different in that the reaction lasts for 240 minutes, the pressure drop of the kettle reaches the preset value of 0.05 MPa, the components of the emulsion terminator are added, the concentration is 40 percent, the oil-soluble terminator comprises the following main components: epoxidized soybean oil, high efficiency terminator, concentration 40%.
Another embodiment is different in that in the above process, the DCS control system precisely controls the feeding and feeding start procedure, when a certain amount of terminator is selected, the advance is set in advance, if the total feeding amount is set to 15.00Kg, when the total feeding amount is 85%, i.e., 12.75 Kg, the valve position of the terminator regulating valve B23 is adjusted to 15%, and when the feeding amount is determined to be 95%, i.e., 14.25 Kg, of the total feeding amount, the terminator cut-off valve B24 and the terminator regulating valve B23 are closed in the adjustment procedure, and the time is delayed for 3-5 minutes after the feeding; when the entering amount is reached, when the entering is finished by 14.70Kg of mass dose, the stop valve cut-off valve 24, the stop agent regulating valve 23 and the stop agent feeding pump 22 are closed in advance, 10Kg of flushing water is added twice respectively, and the dosage of the flushing water is 30.98t after 20 Kg of feeding dose is subtracted from the total amount of the soft water fed by 31.00 t.
The other embodiment is different in that in the above process, any terminator feeding production line is abnormal, the system prompts an alarm prompt message, if the terminator A enters the kettle abnormally, the terminator B line feeding program is automatically started, the difference between the cumulative data A of 14.00Kg and the total amount added of 15.00Kg is 1.00Kg, and the feeding amount of the terminator B line is 1.00 Kg.
The other embodiment is different in that 185 ppm of emulsion terminator is added in the first batch, the time is delayed for 2-3 minutes after the addition, 175ppm of oil-soluble terminator is added, and the time is delayed for 3-5 minutes after the addition; under the condition of stirring at a low speed of 100-110 rpm, the reaction temperature is 57.5 +/-0.2 ℃, and the pressure is 0.68-0.75 MPa.
The other embodiment is different in that 215ppm of emulsion terminator is added into the second batch, 2-3 minutes of delay time is carried out after the addition, and then 225 ppm of oil-soluble terminator is added; stirring at a low speed of 90-100 rpm, wherein the reaction temperature is 57.3 +/-0.2 ℃, and the pressure is 0.68-0.73 MPa; continuously stirring for 5 minutes and discharging.
The application effect shows that the thermal stability of the polyvinyl chloride resin is greatly improved, particularly the aging whiteness index is improved, under the condition that an original terminator is added, the aging whiteness performance index is 79-81, and the aging whiteness performance index is 88-90 after the improvement.
The embodiments of the present invention are described in detail with reference to the prior art, and can be implemented by referring to the prior art. The utility model discloses through the trial and error verification, gained satisfied effect on probation. The above embodiments and examples are specific supports for the technical idea of the implementation method provided by the present invention, and the protection scope of the present invention cannot be limited thereby, and any equivalent changes or equivalent modifications made on the basis of the technical solution according to the technical idea provided by the present invention still belong to the protection scope of the technical solution of the present invention.
Claims (4)
1. A polyvinyl chloride resin heat stability refining production process device is characterized in that: the device comprises a terminator A line, a terminator B line and a kettle inlet line: terminator line a: the device comprises a terminator storage tank A, a terminator feeding pump A, a terminator flow meter A and a terminator regulating valve A which are connected in sequence; a terminator cut-off valve A; terminator line B: the system comprises a terminator storage tank B, a terminator feeding pump B, a terminator flow meter B and a terminator regulating valve B which are connected in sequence; a terminator cutoff valve B; entering a kettle circuit: comprises a kettle feeding pipeline, a feeding main regulating valve, a feeding main cut-off valve and kettle feeding cut-off valves.
2. The apparatus for refining polyvinyl chloride resin with thermal stability as claimed in claim 1, wherein the feeding cut-off valves of each reactor are uniformly distributed on each reactor.
3. The apparatus for refining polyvinyl chloride resin with thermal stability according to claim 1, wherein the stop and start signals of the various components and the feedback signals are introduced into the DCS control system through signal lines.
4. The apparatus for refining and producing polyvinyl chloride resin with thermal stability as claimed in claim 1, wherein the instantaneous metering value and the accumulated metering value of said terminating agent flowmeter A and said terminating agent flowmeter B are introduced into the DCS control system through signal lines.
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